Chinese ephedra medicinal material, and content determination method of three alkaloids in preparation thereof

A determination method and technology of alkaloids, which are applied in the directions of measuring devices, material separation, analysis materials, etc., can solve problems such as the harm of the service life of instruments and chromatographic columns, and increase the operation steps of chromatographic columns. The effect of expansion and cost reduction

Active Publication Date: 2014-01-15
丰宁满族自治县七环旅游开发有限公司
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Problems solved by technology

Moreover, the mobile phases of these medicinal materials and preparations are all phosphate buffered salts that are not recommended under (3) of an appendix VI D of the Chinese Pharmacopoeia version in 2010, and the o

Method used

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  • Chinese ephedra medicinal material, and content determination method of three alkaloids in preparation thereof
  • Chinese ephedra medicinal material, and content determination method of three alkaloids in preparation thereof
  • Chinese ephedra medicinal material, and content determination method of three alkaloids in preparation thereof

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Effect test

Embodiment 1

[0065] (1) Chromatographic conditions and system suitability test: Octadecylsilane bonded silica gel is used as filler; acetonitrile-methanol-0.1% phosphoric acid with volume ratio of 1-1.5:4-4.2:94.5-95.0 is used as mobile phase; Column temperature: 40°C; detection wavelength is 207nm; calculated based on ephedrine hydrochloride peak, it should not be lower than 3000;

[0066] (2) Preparation of reference substance solution Take an appropriate amount of ephedrine hydrochloride, pseudoephedrine hydrochloride and methylephedrine hydrochloride, accurately weighed, add hydrochloric acid-70% methanol solution with a volume ratio of 1: 200, and make every 1ml of ephedrine hydrochloride A solution of 30-15 μg, pseudoephedrine hydrochloride 10-5 μg, and methylephedrine hydrochloride 6-3 μg was used as the reference solution;

[0067](3) Preparation of the test solution: Take 0.2-0.3 g of ephedra medicinal material fine powder, accurately weighed, or 0.5-0.8 g of ephedra preparation, ...

Embodiment 2

[0070] (1) Chromatographic conditions and system suitability test: Octadecylsilane bonded silica gel is used as filler; acetonitrile-methanol-0.1% phosphoric acid with a volume ratio of 1:4.2:94.8 is used as mobile phase; column temperature: 40°C; The detection wavelength is 207nm; calculated according to the peak of ephedrine hydrochloride, it should not be lower than 3000;

[0071] (2) Preparation of the reference substance solution Take appropriate amounts of ephedrine hydrochloride, pseudoephedrine hydrochloride and methylephedrine hydrochloride respectively, accurately weigh them, add hydrochloric acid-70% methanol solution with a volume ratio of 1:200, and make every 1ml of ephedrine hydrochloride A solution of 30 μg of alkali, 10 μg of pseudoephedrine hydrochloride, and 5 μg of methylephedrine hydrochloride is obtained;

[0072] (3) Preparation of the test solution Take 20 tablets of Maxing cough tablets, remove the coating, accurately weigh, grind finely, pass through ...

Embodiment 3

[0075] (1) Chromatographic conditions and system suitability test: Octadecylsilane bonded silica gel is used as filler; acetonitrile-methanol-0.1% phosphoric acid with a volume ratio of 1:4:95 is used as mobile phase; column temperature: 40°C; The detection wavelength is 207nm; calculated according to the peak of ephedrine hydrochloride, it should not be lower than 3000;

[0076] (2) Preparation of the reference substance solution Take appropriate amounts of ephedrine hydrochloride, pseudoephedrine hydrochloride and methylephedrine hydrochloride respectively, accurately weigh them, add hydrochloric acid-70% methanol solution with a volume ratio of 1:200, and make every 1ml of ephedrine hydrochloride A solution of 15 μg of alkali, 5 μg of pseudoephedrine hydrochloride, and 3 μg of methylephedrine hydrochloride is obtained;

[0077] (3) Preparation of the test solution: Take 20 pieces of Jinma Xing cough tablets, remove the coating, accurately weigh, grind, pass through a 50-mes...

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Abstract

The invention relates to a Chinese ephedra medicinal material, and a content determination method of three alkaloids in a preparation thereof. The method has the characteristics that: a common reversed-phase column and a non-buffer salt which is a mobile phase of acetonitrile-methanol-0.1% phosphoric acid with a volume ratio of 1-1.5:4-4.2:94.5-95.0 are adopted; at 207+/-2nm, contents of ephedrine hydrochloride, pseudoephedrine hydrochloride, and ephedrine methyl hydrochloride in the Chinese ephedra medicinal material and the preparation thereof are simultaneously determined. A sample is only processed through water-containing methanol ultrasonic extraction and alumina impurity removing, such that a near-colorless transparent solution is obtained. The method is simple, fast, reproducible, and accurate. According to the quantitative chromatogram of the three alkaloids, a baseline is stable, peak separation is good, and the peak appearing is completed within 20min. Compared with a traditional method with a buffer-salt solution, a specific chromatographic column, and unconventional organic phase ratio and flow rate, with the method provided by the invention, instrument and chromatographic column service lives are prolonged, cost is reduced, and detection conditions are communized. The method is suitable for popularization and application of basic units.

Description

technical field [0001] The invention belongs to the field of quality control of traditional Chinese medicines, and relates to a method for detecting the quality of ephedra medicinal materials and preparations thereof, in particular to a content determination method of three alkaloids in ephedra medicinal materials and preparations thereof. Background technique [0002] Ephedra is the dry herbaceous stem of Ephedra sinica Stapf, Ephedra intermedia Schrenk et C.A. Mey. or Ephedra equisetina Bge. It is a commonly used traditional Chinese medicine in a cough compound preparation. It has the effects of sweating and dispelling cold, clearing the lungs and relieving asthma, diuresis and swelling. For anemofrigid cold, chest tightness, dyspnea and cough, feng shui edema. Honey ephedra nourishes the lungs and relieves cough. Preparations refer to Maxing cough tablets and Jin Maxing cough tablets, both of which are compound preparations for cough relief. The prescription, preparati...

Claims

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Application Information

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IPC IPC(8): G01N30/89G01N30/06G01N30/26
Inventor 韩桂茹张文武安丽娜张文臣申玉龙
Owner 丰宁满族自治县七环旅游开发有限公司
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